scholarly journals Scaling up of continuous-flow, microwave-assisted, organic reactions by varying the size of Pd-functionalized catalytic monoliths

2011 ◽  
Vol 7 ◽  
pp. 1150-1157 ◽  
Author(s):  
Ping He ◽  
Stephen J Haswell ◽  
Paul D I Fletcher ◽  
Stephen M Kelly ◽  
Andrew Mansfield
Keyword(s):  
Flow Reactor ◽  
Flow System ◽  
Operating Conditions ◽  
Microwave Cavity ◽  
Heating Regime ◽  
Reaction Conditions ◽  
Silica Monoliths ◽  
Surface Areas ◽  
Silica Monolith ◽  
Optimal Reaction

A product-scalable, catalytically mediated flow system has been developed to perform Suzuki–Miyaura reactions under a microwave heating regime, in which the volumetric throughput of a Pd-supported silica monolith can be used to increase the quantity of the product without changing the optimal operating conditions. Two silica monoliths (both 3 cm long), with comparable pore diameters and surface areas, were fabricated with diameters of 3.2 and 6.4 mm to give volumetric capacities of 0.205 and 0.790 mL, respectively. The two monoliths were functionalized with a loading of 4.5 wt % Pd and then sealed in heat-shrinkable Teflon® tubing to form a monolithic flow reactor. The Pd-supported silica monolith flow reactor was then placed into the microwave cavity and connected to an HPLC pump and a backpressure regulator to minimize the formation of gas bubbles. The flow rate and microwave power were varied to optimize the reactant contact time and temperature, respectively. Under optimal reaction conditions the quantity of product could be increased from 31 mg per hour to 340 mg per hour simply by changing the volumetric capacity of the monolith.

scholarly journals The direct synthesis of hydrogen peroxide from H 2 and O 2 using Pd–Ni/TiO 2 catalysts

2020 ◽  
Vol 378 (2176) ◽  
pp. 20200062 ◽  
Author(s):  
David A. Crole ◽  
Ricci Underhill ◽  
Jennifer K. Edwards ◽  
Greg Shaw ◽  
Simon J. Freakley ◽  
...  
Keyword(s):  
Hydrogen Peroxide ◽  
Flow Reactor ◽  
Flow System ◽  
Direct Synthesis ◽  
Ni Catalyst ◽  
Batch Experiments ◽  
Reaction Conditions ◽  
Ambient Temperatures ◽  
Degradation Reactions ◽  
Means Of Production

The direct synthesis of hydrogen peroxide (H 2 O 2 ) from molecular H 2 and O 2 offers an attractive, decentralized alternative to production compared to the current means of production, the anthraquinone process. Herein we evaluate the performance of a 0.5%Pd–4.5%Ni/TiO 2 catalyst in batch and flow reactor systems using water as a solvent at ambient temperature. These reaction conditions are considered challenging for the synthesis of high H 2 O 2 concentrations, with the use of sub-ambient temperatures and alcohol co-solvents typical. Catalytic activity was observed to be stable to prolonged use in multiple batch experiments or in a flow system, with selectivities towards H 2 O 2 of 97% and 85%, respectively. This study was carried out in the absence of halide or acid additives that are typically used to inhibit sequential H 2 O 2 degradation reactions showing that this Pd–Ni catalyst has the potential to produce H 2 O 2 selectively. This article is part of a discussion meeting issue ‘Science to enable the circular economy’.

Synthesis of Phosphonates via Michaelis-Arbuzov Reaction

2017 ◽  
Vol 14 (6) ◽  
pp. 883-903 ◽  
Author(s):  
Boppudi Hari Babu ◽  
Gandavaram Syam Prasad ◽  
Chamarthi Naga Raju ◽  
Mandava Venkata Basaveswara Rao
Keyword(s):  
Reaction Times ◽  
Biologically Active ◽  
Fine Tuning ◽  
Arbuzov Reaction ◽  
Reaction Conditions ◽  
Solvent Type ◽  
Potential Applications ◽  
Synthetic Methodologies ◽  
Optimal Reaction ◽  
The Arbuzov Reaction

Background: Michaelis–Arbuzov reaction has played a key role for the synthesis of dialkyl or diaryl phosphonates by reacting various alkyl or aryl halides with trialkyl or triaryl phosphite. This reaction is very versatile in the formation of P-C bond from the reaction of aliphatic halides with phosphinites or phosphites to yield phosphonates, phosphinates, phosphine oxides. The Arbuzov reaction developed some methodologies, possible mechanistic pathways, selectivity, potential applications and biologically active various phosphonates. Objective: The synthesis of phosphonates via Michaelis–Arbuzov reaction with many new and fascinating methodologies were developed and disclosed in the literature, and these are explored in this review. Conclusion: This review has discussed past developments and vast potential applications of Arbuzov reaction in the synthesis of organophosphonates. As presented in this review, various synthetic methodologies were developed to prepare a large variety of phosphonates. Improvements in the reaction conditions of Lewis-acid mediated Arbuzov rearrangement as well as the development of MW-assisted Arbuzov rearrangement were discussed. Finally, to achieve high selectivities and yields, fine-tuning of reaction conditions including solvent type, temperature, and optimal reaction times to be considered.

Amperometric assay of vitamin C using an ascorbate oxidase enzyme electrode

1979 ◽  
Vol 44 (11) ◽  
pp. 3395-3404 ◽  
Author(s):  
Pavel Posádka ◽  
Lumír Macholán
Keyword(s):  
Ascorbic Acid ◽  
Vitamin C ◽  
Oxygen Electrode ◽  
Ascorbate Oxidase ◽  
Current Response ◽  
Reaction Conditions ◽  
Long Term Storage ◽  
Oxidase Enzyme ◽  
Optimal Reaction

An oxygen electrode of the Clark type, coated by a thin, active layer of chemically insolubilized ascorbate oxidase from squash peelings specifically detects by measuring oxygen uptake 10 to 400 μg of ascorbic acid in 3 ml of phosphate buffer. The record of current response to substrate addition lasts 1-2 min. The ascorbic acid values determined in various samples of fruit juices are in good agreement with the data obtained by titration and polarography. The suitable composition of the membrane and its lifetime and stability during long-term storage are described; optimal reaction conditions of vitamin C determination and the possibilities of interference of other compounds are also examined. Of the 35 phenols, aromatic amines and acids tested chlorogenic acid only can cause a positive error provided that the enzyme membrane has been prepared from ascorbate oxidase of high purity.

scholarly journals A Novel Pseudomonas geniculata AGE Family Epimerase/Isomerase and Its Application in d-Mannose Synthesis

Foods ◽  
2020 ◽  
Vol 9 (12) ◽  
pp. 1809
Author(s):  
Zhanzhi Liu ◽  
Ying Li ◽  
Jing Wu ◽  
Sheng Chen
Keyword(s):  
3D Structure ◽  
Three Dimensional ◽  
Optimal Temperature ◽  
Reaction Conditions ◽  
Enzymatic Production ◽  
Physiological Properties ◽  
Potential Applications ◽  
Kinetics Of ◽  
Optimal Reaction ◽  
Gene Age

d-mannose has exhibited excellent physiological properties in the food, pharmaceutical, and feed industries. Therefore, emerging attention has been applied to enzymatic production of d-mannose due to its advantage over chemical synthesis. The gene age of N-acetyl-d-glucosamine 2-epimerase family epimerase/isomerase (AGEase) derived from Pseudomonas geniculata was amplified, and the recombinant P. geniculata AGEase was characterized. The optimal temperature and pH of P. geniculata AGEase were 60 °C and 7.5, respectively. The Km, kcat, and kcat/Km of P. geniculata AGEase for d-mannose were 49.2 ± 8.5 mM, 476.3 ± 4.0 s−1, and 9.7 ± 0.5 s−1·mM−1, respectively. The recombinant P. geniculata AGEase was classified into the YihS enzyme subfamily in the AGE enzyme family by analyzing its substrate specificity and active center of the three-dimensional (3D) structure. Further studies on the kinetics of different substrates showed that the P. geniculata AGEase belongs to the d-mannose isomerase of the YihS enzyme. The P. geniculata AGEase catalyzed the synthesis of d-mannose with d-fructose as a substrate, and the conversion rate was as high as 39.3% with the d-mannose yield of 78.6 g·L−1 under optimal reaction conditions of 200 g·L−1d-fructose and 2.5 U·mL−1P. geniculata AGEase. This novel P. geniculata AGEase has potential applications in the industrial production of d-mannose.

scholarly journals Efficient Degradation of Mordant Blue 9 Using the Fenton-Activated Persulfate System

Water ◽  
2019 ◽  
Vol 11 (12) ◽  
pp. 2532 ◽  
Author(s):  
Md. Nahid Pervez ◽  
Felix Y. Telegin ◽  
Yingjie Cai ◽  
Dongsheng Xia ◽  
Tiziano Zarra ◽  
...  
Keyword(s):  
Butyl Alcohol ◽  
Textile Dye ◽  
Oh Radicals ◽  
Operational Parameters ◽  
Reaction Conditions ◽  
Tert Butyl Alcohol ◽  
Initial Ph ◽  
Fe Complex ◽  
Optimal Reaction ◽  
Activated Persulfate

In this study, a Fenton-activated persulfate (Fe2+/PS) system was introduced for the efficient degradation of Mordant Blue 9 (MB 9) as a textile dye in an aqueous solution. Results showed that the degradation of MB 9 was markedly influenced by operational parameters, such as initial pH, PS concentration, Fe2+ concentration, and initial dye concentration. Optimal reaction conditions were then determined. Inorganic anions, such as Cl− and HCO3−, enhanced the degradation efficiency of MB 9 under optimal conditions. Addition of HCO3− reduced the degradation performance of MB 9, whereas the addition of Cl− increased the degradation percentage of MB 9. In addition, quenching experiments were conducted using methanol and tert-butyl alcohol as scavengers, and methanol was identified as an effective scavenger. Thus, the degradation of MB 9 was attributed to S O 4 • − and •OH radicals. The degradation and mineralization efficiency of MB 9 was significantly reduced using the conventional Fenton process i.e., Fe2+/ hydrogen peroxide (HP) because of the formation of a Fe complex during degradation. Meanwhile, the Fe2+/persulfate (PS) system improved the degradation and mineralization performance.

scholarly journals Software-guided microscale flow calorimeter for efficient acquisition of thermokinetic data

2021 ◽  
Author(s):  
Timothy Aljoscha Frede ◽  
Marlene Dietz ◽  
Norbert Kockmann
Keyword(s):  
Design Of Experiments ◽  
Process Development ◽  
Reaction Conditions ◽  
Experimental Conditions ◽  
Flow Calorimeter ◽  
Microscale Flow ◽  
Increased Sensitivity ◽  
Important Time ◽  
Optimal Reaction

AbstractFast chemical process development is inevitably linked to an optimized determination of thermokinetic data of chemical reactions. A miniaturized flow calorimeter enables increased sensitivity when examining small amounts of reactants in a short time compared to traditional batch equipment. Therefore, a methodology to determine optimal reaction conditions for calorimetric measurement experiments was developed and is presented in this contribution. Within the methodology, short-cut calculations are supplemented by computational fluid dynamics (CFD) simulations for a better representation of the hydrodynamics within the microreactor. This approach leads to the effective design of experiments. Unfavourable experimental conditions for kinetics experiments are determined in advance and therefore, need not to be considered during design of experiments. The methodology is tested for an instantaneous acid-base reaction. Good agreement of simulations was obtained with experimental data. Thus, the prediction of the hydrodynamics is enabled and the first steps towards a digital twin of the calorimeter are performed. The flow rates proposed by the methodology are tested for the determination of reaction enthalpy and showed that reasonable experimental settings resulted. Graphical abstract A methodology is suggested to evaluate optimal reaction conditions for efficientacquisition of kinetic data. The experimental design space is limited by thestepwise determination of important time scales based on specified input data.

The Influences of Reaction Conditions on Phenanthrene Hydrogenation over NiW/Al2O3 Catalyst

2012 ◽  
Vol 512-515 ◽  
pp. 2200-2206
Author(s):  
Kun Wang ◽  
Jun Guan ◽  
De Min He ◽  
Qiu Min Zhang
Keyword(s):  
Positive Impact ◽  
Volume Ratio ◽  
Operating Conditions ◽  
Reaction Conditions ◽  
Remarkable Effect ◽  
Ms Analysis ◽  
Temperature And Pressure ◽  
Cracking Products

Hydrogenation of phenanthrene (PHE HYD) was investigated over a commercial NiW/Al2O3catalyst under practical reaction conditions. GC-MS analysis was utilized to identify the numerous products formed during PHE HYD. The products included dihydrophenanthrene (DHP), 1,2,3,4-tetrahydrophenanthrene (THP), sym-octahydrophenanthrene (1,8-OHP), asym-octahydrophenanthrene (1,10-OHP) and perhydrophenanthrene (PHP), but the cracking products were not found under the reaction conditions. The effects of operating conditions such as temperature, pressure and H2/liquor on PHE HYD were tested in detail. It is found that temperature and pressure had remarkable effect on PHE HYD, but volume ratio of H2/liquor had little effect on PHE HYD at the observation range. The addition of decalin had a positive impact on PHE HYD; it could increase the conversion of PHE and the selectivity to PHP.

scholarly journals Synthesis of propylene carbonate from urea and 1,2-propylene glycol over metal carbonates

2011 ◽  
Vol 17 (3) ◽  
pp. 323-331 ◽  
Author(s):  
Jiancheng Zhou ◽  
Wu Dongfang ◽  
Birong Zhang ◽  
Yali Guo
Keyword(s):  
Reaction Time ◽  
Propylene Glycol ◽  
Propylene Carbonate ◽  
Reaction Temperature ◽  
Reaction Conditions ◽  
Lead Carbonate ◽  
Synthetic Process ◽  
Metal Carbonates ◽  
Optimal Reaction ◽  
Mixed Carbonate

A series of single-metal carbonates and Pb-Zn mixed-metal carbonates were prepared as catalysts for alcoholysis of urea with 1,2-propylene glycol (PG) for the synthesis of propylene carbonate (PC). The mixed carbonates all show much better catalytic activities than the single carbonates, arising from a strong synergistic effect between the two crystalline phases, hydrozincite and lead carbonate. The mixed carbonate with Pb/Zn=1:2 gives the highest yield of PC, followed by the mixed carbonate with Pb/Zn=1:3. Furthermore, Taguchi method was used to optimize the synthetic process for improving the yield of PC. It is shown that the reaction temperature is the most significant factor affecting the yield of PC, followed by the reaction time, and that the optimal reaction conditions are the reaction time at 5 hours, the reaction temperature at 180 oC and the catalyst amount at 1.8 wt%, resulting in the highest PC yield of 96.3%.

scholarly journals Evaluation of wet air oxidation variables for removal of organophosphorus pesticide malathion using Box-Behnken design

2016 ◽  
Vol 75 (3) ◽  
pp. 619-628 ◽  
Author(s):  
Melike Isgoren ◽  
Erhan Gengec ◽  
Sevil Veli
Keyword(s):  
Removal Efficiency ◽  
Applied Pressure ◽  
Organophosphorus Pesticide ◽  
Operating Conditions ◽  
Quadratic Model ◽  
Air Oxidation ◽  
Wet Air Oxidation ◽  
Reaction Conditions ◽  
Efficient Treatment ◽  
Optimum Reaction

This paper deals with finding optimum reaction conditions for wet air oxidation (WAO) of malathion aqueous solution, by Response Surface Methodology. Reaction conditions, which affect the removal efficiencies most during the non-catalytic WAO system, are: temperature (60–120 °C), applied pressure (20–40 bar), the pH value (3–7), and reaction time (0–120 min). Those were chosen as independent parameters of the model. The interactions between parameters were evaluated by Box-Behnken and the quadratic model fitted very well with the experimental data (29 runs). A higher value of R2 and adjusted R2 (>0.91) demonstrated that the model could explain the results successfully. As a result, optimum removal efficiency (97.8%) was obtained at pH 5, 20 bars of pressure, 116 °C, and 96 min. These results showed that Box–Behnken is a suitable design to optimize operating conditions and removal efficiency for non-catalytic WAO process. The EC20 value of raw wastewater was measured as 35.40% for malathion (20 mg/L). After the treatment, no toxicity was observed at the optimum reaction conditions. The results show that the WAO is an efficient treatment system for malathion degradation and has the ability of converting malathion to the non-toxic forms.

Optimization of biodiesel synthesis under simultaneous ultrasound-microwave irradiation using response surface methodology (RSM)

2015 ◽  
Vol 4 (4) ◽  
Author(s):  
Seyed Mohammad Safieddin Ardebili ◽  
Teymor Tavakoli Hashjin ◽  
Barat Ghobadian ◽  
Gholamhasan Najafi ◽  
Stefano Mantegna ◽  
...  
Keyword(s):  
Response Surface Methodology ◽  
Microwave Irradiation ◽  
Response Surface ◽  
Palm Oil ◽  
Catalyst Concentration ◽  
Irradiation Time ◽  
Operating Conditions ◽  
Molar Ratio ◽  
Reaction Conditions ◽  
Biodiesel Synthesis

AbstractThis work investigates the effect of simultaneous ultrasound-microwave irradiation on palm oil transesterification and uncovers optimal operating conditions. Response surface methodology (RSM) has been used to analyze the influence of reaction conditions, including methanol/palm oil molar ratio, catalyst concentration, reaction temperature and irradiation time on biodiesel yield. RSM analyses indicate 136 s and 129 s as the optimal sonication and microwave irradiation times, respectively. Optimized parameters for full conversion (97.53%) are 1.09% catalyst concentration and a 7:3.1 methanol/oil molar ratio at 58.4°C. Simultaneous ultrasound-microwave irradiation dramatically accelerates the palm oil transesterification reaction. Pure biodiesel was obtained after only 2.2 min while the conventional method requires about 1 h.

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